CN104051790B - A kind of method being prepared lithium battery by garlic and/or onion - Google Patents
A kind of method being prepared lithium battery by garlic and/or onion Download PDFInfo
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- CN104051790B CN104051790B CN201410249563.4A CN201410249563A CN104051790B CN 104051790 B CN104051790 B CN 104051790B CN 201410249563 A CN201410249563 A CN 201410249563A CN 104051790 B CN104051790 B CN 104051790B
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- 240000002234 Allium sativum Species 0.000 title claims abstract description 43
- 235000004611 garlic Nutrition 0.000 title claims abstract description 43
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 35
- 241000234282 Allium Species 0.000 title claims abstract description 29
- 235000002732 Allium cepa var. cepa Nutrition 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 40
- 239000000341 volatile oil Substances 0.000 claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000003763 carbonization Methods 0.000 claims abstract description 11
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 11
- 239000007772 electrode material Substances 0.000 claims abstract description 10
- 210000002615 epidermis Anatomy 0.000 claims abstract description 10
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 239000004020 conductor Substances 0.000 claims abstract description 9
- 239000011244 liquid electrolyte Substances 0.000 claims abstract description 9
- 238000004132 cross linking Methods 0.000 claims abstract description 5
- 238000007259 addition reaction Methods 0.000 claims abstract description 3
- 235000013372 meat Nutrition 0.000 claims abstract description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 10
- -1 allyl methyl thioether Chemical compound 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- XNZOTQPMYMCTBZ-UHFFFAOYSA-N allyl methyl disulfide Chemical compound CSSCC=C XNZOTQPMYMCTBZ-UHFFFAOYSA-N 0.000 claims description 4
- PFRGXCVKLLPLIP-UHFFFAOYSA-N diallyl disulfide Chemical compound C=CCSSCC=C PFRGXCVKLLPLIP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- YDNYEJZZJXFADP-SNVBAGLBSA-N (2r)-5-amino-2-[(4-methylphenyl)sulfonylamino]-5-oxopentanoic acid Chemical compound CC1=CC=C(S(=O)(=O)N[C@H](CCC(N)=O)C(O)=O)C=C1 YDNYEJZZJXFADP-SNVBAGLBSA-N 0.000 claims description 2
- VNFYMAPAENTMMO-UHFFFAOYSA-N 5-chloro-2-methylquinoline Chemical compound ClC1=CC=CC2=NC(C)=CC=C21 VNFYMAPAENTMMO-UHFFFAOYSA-N 0.000 claims description 2
- JGMPRNFEEAJLAJ-UHFFFAOYSA-N allyl methyl trisulphide Natural products CSSSCC=C JGMPRNFEEAJLAJ-UHFFFAOYSA-N 0.000 claims description 2
- 229940008075 allyl sulfide Drugs 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 229910003002 lithium salt Inorganic materials 0.000 claims 2
- 159000000002 lithium salts Chemical class 0.000 claims 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 9
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 3
- JDLKFOPOAOFWQN-VIFPVBQESA-N Allicin Natural products C=CCS[S@](=O)CC=C JDLKFOPOAOFWQN-VIFPVBQESA-N 0.000 description 8
- JDLKFOPOAOFWQN-UHFFFAOYSA-N allicin Chemical compound C=CCSS(=O)CC=C JDLKFOPOAOFWQN-UHFFFAOYSA-N 0.000 description 8
- 235000010081 allicin Nutrition 0.000 description 8
- 239000003792 electrolyte Substances 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 5
- 239000005030 aluminium foil Substances 0.000 description 5
- 238000009837 dry grinding Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000001238 wet grinding Methods 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052493 LiFePO4 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 238000000935 solvent evaporation Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- General Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of method being prepared lithium battery by garlic and/or onion, the method be with garlic and/or onion for raw material, garlic and/or onion epidermis are obtained the active carbon as electrode conductive material by high temperature carbonization; Using the essential oil that the meat of garlic and/or onion obtains as binders for electrodes and/or liquid electrolyte material by alcohol extract; Essential oil is carried out further the modified polyorganosiloxane that addition reaction obtains as solid electrolyte material with poly-methylhydrogen silicone, or crosslinking curing obtains the solidfied material as electrode active material further; Allocate one or more in the described active carbon obtained for raw material with garlic and/or onion, essential oil, modified polyorganosiloxane, solidfied material into other stock preparing lithium battery and be prepared into solid-state or liquid lithium battery; This preparation method is simple, cost is low, and obtained lithium battery capacity is large, good cycle, expands range of choice and the application of lithium ion battery material.
Description
Technical field
The present invention relates to a kind of method being prepared lithium battery by garlic and/or onion, belong to lithium ion battery material technology of preparing and application thereof.
Background technology
Lithium ion battery has that energy density is high, the feature of long service life, got most of the attention since putting goods on the market from 1991 always, be widely used in middle-size and small-size field of batteries such as mobile phone, notebook computer, electric tool, electric bicycles, become in the 21 century economy of energy an indispensable part.But, in recent years, the rise of electric motor car, high-power, high-capacity secondary battery demand are increasingly sharpened, more and more higher to the requirement of lithium ion battery material and lithium ion battery production technology, continually develop and have high storage density, safe and reliable, cheap lithium ion battery material, one-step optimization production technology etc. of going forward side by side has become the developing direction of lithium ion battery industry.
Natural plant resource is abundanter, a lot of example active carbon being prepared by natural plant fibre is had in prior art, as publication number (CN102951635A) discloses a kind of method utilizing wooden slag and tealeaves charing to prepare active carbon, its active carbon prepared is mainly used to the moisture absorption, inhales taste.The natural botanical source such as garlic, onion is abundant, and the plant such as garlic, onion has abundant string simultaneously, is rich in organic sulfur compound.Galic essential oil is described as wide-spectrum bactericide, and have the feature of integration of drinking and medicinal herbs, doctor's food homology, it is still a kind of flavouring not, has unique fragrant pungent, the more important thing is that it has broad-spectrum sterilization effect, due to its multiple effect pharmacologically.Publication number (CN102311879A) discloses a kind of preparation method of galic essential oil, specifically adopts molecular clock separation and purification.If the plant resources that garlic, onion etc. are abundant can be made full use of field of lithium by imagination, expansion battery material selection range, reduction material cost tool are of great significance.
Summary of the invention
The object of the invention is to be that providing a kind of utilizes cheap natural plants to be raw material, prepared the method for lithium ion battery of high power capacity, low cost by easy steps.
The invention provides a kind of method being prepared lithium battery by garlic and/or onion, the method be with garlic and/or onion for raw material, garlic and/or onion epidermis are obtained the active carbon as electrode conductive material by 550 ~ 650 DEG C of high temperature carbonizations; Using the essential oil that the meat of garlic and/or onion obtains as binders for electrodes and/or liquid electrolyte material by alcohol extract; Using the modified polyorganosiloxane that described essential oil carries out addition reaction with poly-methylhydrogen silicone obtain as solid electrolyte material at 70 ~ 90 DEG C further; Or using described essential oil further at 55 ~ 65 DEG C of temperature crosslinking curing obtain the solidfied material as electrode active material; By the described active carbon, essential oil, modified polyorganosiloxane, one or more in solidfied material that obtain for raw material with garlic and/or onion, allocate other stock preparing lithium battery into and be prepared into solid-state or liquid lithium battery.
The method preparing lithium battery by garlic and/or onion of the present invention also comprises following preferred version.
In preferred method by the active carbon that obtains for raw material using garlic and/or onion as electrode conductive material, obtained essential oil as binders for electrodes and/or liquid electrolyte material, obtained modified polyorganosiloxane as solid electrolyte material and obtained solidfied material as electrode active material, allocate other stock preparing lithium battery into and be prepared into solid-state or liquid lithium battery.Most preferably be with garlic be the active carbon that obtains of raw material as electrode conductive material, obtained essential oil as binders for electrodes and as liquid electrolyte material and obtained solidfied material as electrode active material, allocate other stock preparing lithium battery into and be prepared into liquid lithium battery; Or taking garlic as the active carbon that obtains of raw material as electrode active material, allocates other stock preparing lithium battery into and is prepared into solid state lithium battery as binders for electrodes, obtained modified polyorganosiloxane as solid electrolyte material and obtained solidfied material as electrode conductive material, obtained essential oil.
Essential oil described in preferred method comprises the organic compounds containing sulfur of allyl methyl thioether, allyl sulfide, allyl methyl disulfide, diallyl disulphide, allyl methyl trisulfide ether, Diallytrisin and Diallytrisin.
In preferred method, garlic and/or onion remove epidermis, are smashed to pieces by pulp, dry moisture at 55 ~ 65 DEG C after, grinding, gained powder ethanol soaks 4 ~ 8h at 40 ~ 50 DEG C, suction filtration, obtain extract, gained extract evaporate to dryness alcohol solvent, obtains essential oil.
In preferred method, garlic and/or onion epidermis are under an inert atmosphere, carbonize 18 ~ 30h, obtain active carbon under 550 ~ 650 DEG C of high temperature.
The time of crosslinking curing described in preferred method is 64 ~ 80h.
Essential oil described in preferred method and poly-methylhydrogen silicone are dissolved in benzene kind solvent in 1:3 ~ 5 in mass ratio, react 20 ~ 28h, obtain modified polyorganosiloxane at the temperature of 70 ~ 90 DEG C.
Described benzene kind solvent is toluene, dimethylbenzene etc.
Beneficial effect of the present invention: the present invention prepares electrodes conduct absorbent charcoal material using the natural plant raw material such as garlic, onion first by straightforward procedure, can be used as the essential oil of binders for electrodes and/or liquid electrolyte material, can be used as the modified polyorganosiloxane of solid electrolyte material and the solidfied material as electrode active material, select wherein one or more allocate other stock preparing lithium battery again into and be prepared into solid-state or liquid lithium battery; Conduction active-carbon, binding agent, electrolyte and the electrode active material most preferably be in solid-state or liquid lithium battery is all prepared by garlic raw material, obtained lithium battery capacity is large, good cycle, cost is low, expands range of choice and the application of lithium ion battery material.
Accompanying drawing explanation
The lithium battery cycle performance figure that [Fig. 1] obtains for the embodiment of the present invention 1.
The lithium battery cycle performance figure that [Fig. 1] obtains for the embodiment of the present invention 2.
Embodiment
Following examples are intended to further illustrate content of the present invention, instead of limit the scope of the invention.
Embodiment 1
By garlic peeling, be pounded mashed garlic, put into baking oven, dry 6h at 60 DEG C, grinds, adds absolute ethyl alcohol, and soak 6h at 50 DEG C, suction filtration, clear liquid is allicin ethanol stoste, and evaporate to dryness allicin solution obtains galic essential oil.Take the sublimed sulfur of the galic essential oil of 0.05g, the conductive black of 0.15g and 0.3g, mix, fully grind.Batch mixing after dry grinding is that solvent carries out wet-milling with 1-METHYLPYRROLIDONE.Slurry after milled is coated on aluminium foil, drying two days at the temperature of 60 DEG C.Dried pole piece is cut into the disk that diameter is 1cm.With this disk for positive pole, metal organic frame is the polyoxyethylene solid electrolyte of filler is electrolyte, and lithium sheet is negative pole, is assembled into button cell, carries out charge-discharge test.Battery 80 DEG C and 0.3C multiplying power cycle performance as shown in Figure 1.
Embodiment 2
By garlic peeling, be pounded mashed garlic, put into baking oven, dry 7h at 60 DEG C, grinds, adds absolute ethyl alcohol, and soak 6h at 45 DEG C, suction filtration, clear liquid is allicin ethanol stoste, and evaporate to dryness allicin solution obtains galic essential oil.The poly-methylhydrogen silicone of the galic essential oil of 0.5g and 2g is dissolved in toluene, 80 DEG C of back flow reaction 26h, product is carried out revolving evaporate to dryness dry, except desolventizing, obtain the polysiloxanes of galic essential oil modification.This polysiloxanes of 0.5g and the LiTFSI of 0.1g are dissolved in acetonitrile, use solvent evaporation method to be prepared into copolymer solid electrolyte.Take LiFePO4 as positive pole, lithium sheet is negative pole, uses this electrolyte to assemble button cell, carries out charge-discharge test.Battery 80 DEG C and 1C multiplying power cycle performance as shown in Figure 2.
Embodiment 3
The epidermis of fresh garlic is placed in tube furnace, carries out carbonization under an argon atmosphere to it, temperature is 600 DEG C, and carbonization time is 24h, obtains black bar material.Get the material after the carbonization of 0.15g, the Kynoar of 0.05g and the sublimed sulfur of 0.3g, carry out mixing and fully grinding, be that solvent carries out wet-milling with 1-METHYLPYRROLIDONE after dry grinding, the slurry after milled is coated on aluminium foil, drying two days at the temperature of 60 DEG C.Dried pole piece is cut into the disk that diameter is 1cm.With this disk for positive pole, metal organic frame is the polyoxyethylene solid electrolyte of filler is electrolyte, and lithium sheet is negative pole, is assembled into button cell, carries out charge-discharge test, and battery is 830mAhg in the initial discharge specific capacity of 80 DEG C and 0.3C circulation
-1.
Embodiment 4
The epidermis of fresh garlic is placed in tube furnace, carries out carbonization under an argon atmosphere to it, temperature is 600 DEG C, and carbonization time is 28h, obtains black bar material.Obtain galic essential oil by the method identical with embodiment 2, and be prepared into copolymer solid electrolyte.Get the material after the carbonization of 0.15g, the Kynoar of 0.05g and the LiFePO4 of 0.3g, carry out mixing and fully grinding, be that solvent carries out wet-milling with 1-METHYLPYRROLIDONE after dry grinding, the slurry after milled is coated on aluminium foil, drying two days at the temperature of 60 DEG C.Dried pole piece is cut into the disk that diameter is 1cm.With this disk for positive pole, the copolymer solid electrolyte of preparation is electrolyte, and lithium sheet is negative pole, is assembled into button cell, carries out charge-discharge test, and battery is 135mAhg in the initial discharge specific capacity of 80 DEG C and 0.3C circulation
-1, after circulation 20 circle, capability retention is 99.5%.
Embodiment 5
By garlic peeling, be pounded mashed garlic, put into baking oven, dry 8h at 60 DEG C, grinds, adds absolute ethyl alcohol, and soak 6h at 40 DEG C, suction filtration, clear liquid is allicin ethanol stoste, and evaporate to dryness allicin solution obtains galic essential oil.Galic essential oil is placed in 60 DEG C and heats 72h, obtain solid product.Take this product of 0.3g, the Kynoar of 0.05g and the conductive black of 0.15g, mix, fully grind.Batch mixing after dry grinding is that solvent carries out wet-milling with 1-METHYLPYRROLIDONE.Slurry after milled is coated on aluminium foil, drying two days at the temperature of 60 DEG C.Dried pole piece is cut into the disk that diameter is 1cm.With this disk for positive pole, metal organic frame is the polyoxyethylene solid electrolyte of filler is electrolyte, and lithium sheet is negative pole, is assembled into button cell, carries out charge-discharge test, and battery is 310mAhg in the initial discharge specific capacity of 80 DEG C and 0.3C circulation
-1, after circulation 20 circle, capability retention is 98.6%.
Embodiment 6
By garlic peeling, be pounded mashed garlic, put into baking oven, dry 6h at 60 DEG C, grinds, adds absolute ethyl alcohol, and soak 6h at 50 DEG C, suction filtration, clear liquid is allicin ethanol stoste, and evaporate to dryness allicin solution obtains galic essential oil.Galic essential oil is placed in 60 DEG C and heats 72h, obtain solid product, as electrode active material.The poly-methylhydrogen silicone of the galic essential oil of 0.5g and 2g is dissolved in toluene, 80 DEG C of back flow reaction 24h, product is carried out revolving evaporate to dryness dry, except desolventizing, obtain the polysiloxanes of galic essential oil modification.This polysiloxanes of 0.5g and the LiTFSI of 0.1g are dissolved in acetonitrile, use solvent evaporation method to be prepared into galic essential oil modified polyorganosiloxane solid electrolyte.The epidermis of fresh garlic is placed in tube furnace, carries out carbonization under an argon atmosphere to it, temperature is 600 DEG C, and carbonization time is 20h, obtains black bar material, as electrode conductive material.Get the electric conducting material of the active material of 0.3g, the galic essential oil of 0.05g and 0.15g, mix, fully grind.Batch mixing after dry grinding is that solvent carries out wet-milling with 1-METHYLPYRROLIDONE.Slurry after milled is coated on aluminium foil, drying two days at the temperature of 60 DEG C.Dried pole piece is cut into the disk that diameter is 1cm.With this disk for positive pole, galic essential oil modified polyorganosiloxane solid electrolyte is electrolyte, and lithium sheet is negative pole, is assembled into button cell, carries out charge-discharge test, battery in the initial discharge specific capacity of 80 DEG C and 0.3C circulation close to 300mAhg
-1, after circulation 20 circle, capability retention is 98.8%.
Claims (8)
1. prepared a method for lithium battery by garlic and/or onion, it is characterized in that, with garlic and/or onion for raw material, garlic and/or onion epidermis are obtained the active carbon as electrode conductive material by 550 ~ 650 DEG C of high temperature carbonizations; Using the essential oil that the meat of garlic and/or onion obtains as binders for electrodes and/or liquid electrolyte material by alcohol extract; Using the modified polyorganosiloxane that described essential oil carries out addition reaction with poly-methylhydrogen silicone obtain as solid electrolyte material at 70 ~ 90 DEG C further; Or using described essential oil further at 55 ~ 65 DEG C of temperature crosslinking curing obtain the solidfied material as electrode active material; By the described active carbon, essential oil, modified polyorganosiloxane, one or more in solidfied material that obtain for raw material with garlic and/or onion, allocate other stock preparing lithium battery into and be prepared into solid-state or liquid lithium battery.
2. the method for claim 1, it is characterized in that, by the active carbon that obtains for raw material using garlic and/or onion as electrode conductive material, obtained essential oil as binders for electrodes and/or liquid electrolyte material, obtained modified polyorganosiloxane as solid electrolyte material, with obtained solidfied material as electrode active material, allocate other stock preparing lithium battery into and be prepared into solid-state or liquid lithium battery.
3. method as claimed in claim 1 or 2, it is characterized in that, described essential oil comprises the organic compounds containing sulfur of allyl methyl thioether, allyl sulfide, allyl methyl disulfide, diallyl disulphide, allyl methyl trisulfide ether, Diallytrisin and Diallytrisin.
4. method as claimed in claim 1 or 2, it is characterized in that, garlic and/or onion remove epidermis, are smashed to pieces by pulp, dry moisture at 55 ~ 65 DEG C after, grinding, gained powder ethanol soaks 4 ~ 8h at 40 ~ 50 DEG C, and suction filtration, obtains extract, gained extract evaporate to dryness alcohol solvent, obtains essential oil.
5. method as claimed in claim 1 or 2, is characterized in that, garlic and/or onion epidermis under an inert atmosphere, carbonize 18 ~ 30h, obtain active carbon under 550 ~ 650 DEG C of high temperature.
6. the method for claim 1, is characterized in that, the time of described crosslinking curing is 64 ~ 80h.
7. method as claimed in claim 1 or 2, it is characterized in that, described essential oil and poly-methylhydrogen silicone are dissolved in benzene kind solvent in 1:3 ~ 5 in mass ratio, react 20 ~ 28h, obtain modified polyorganosiloxane at the temperature of 70 ~ 90 DEG C; Described benzene kind solvent is toluene or dimethylbenzene.
8. method as claimed in claim 1 or 2, it is characterized in that, described modified polyorganosiloxane is mixed to get solid electrolyte as solid electrolyte material and lithium salts, and described essential oil is directly mixed to get liquid electrolyte as liquid electrolyte material and lithium salts.
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| CN102311879A (en) * | 2010-07-08 | 2012-01-11 | 朱茂松 | Preparation method of separated and purified garlic essence |
| RU2488558C2 (en) * | 2011-09-01 | 2013-07-27 | Общество С Ограниченной Ответственностью "Рисилика" | Method of producing high-purity amorphous microsilica from rice husks |
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